Organic phosphorus compound and process of making same.



UNITED STATES P TENT Unseen} I Patented March 1 5, 1904. I i

- SWIGE L POSTERNAK, OF BEENDON, FRANCE.

ORGANIC PHosPH'oRus COMPOUND- pp PnooE'ss oF'mAkmo. SAME.

SPECIFICATION forming part of Letters Patent No. 754,803, dated March 15, 1904.

Application filed Mai-oh 21, 1902.

T all whmn it may concern:. 7

Be it known that 'I, SWIGEL PosTERNAK, a sub ect of the Emperor of Russia, residing at Place Rabelais 2, Mendon, France, have inplants.

vented certain newfiand useful Improvements in Obtaining Foods'tufis, of which the following is a specification.

This invention relates to a process for obtaining the organic-phosphorus compound contained in most vegetable foodstuffs, which is ieposited as a; ndependent phosphorus reserve material incotyledons or tubercules, rhicomes, and the like ofall cholorophyll The said organic phosphorus compound possesses the chemical constitution C liePzOt, and as the latest experiments have shown it can be considered according to the grouping of its atoms as-an anhydrooxyme-- thylendiphosphoric acid. The process for obtaining this substance hereinafter described is based upon the observation that this organic phosphorus compound is readily soluble in weak mineral acids in the presence of earth alkalies usually'found in plants and that the vegetable albumen in the presence of suificient qua-n t-ities of the above phosphorus compound 'is 'quite insoluble -in diluted mineral acids and, moreover, upon the property of mineral acid extracts from plant seeds or oil-cakes, which consists in the fact that the organic phosphorus compound contained in these extracts is precipitated in the for'm of double salts of 'a metal base and of the alkaline earths, if to the extracts there is added a salt of a metal belonging principally to the copper group and if the free mineral acid is replaced by an organic acicl by means of double decomposition with an organic alkali salt.

The process is carried out in the following manner with oil-cake, which is best suited for the purpose: One hundred kilograms of well pulverized oil-cake is stirred'with three huntreatment. After two hours from six to seven .Serisl Ho. 99,367. (Specimens) liters commercial hydrochloric acid is added to the liquid and the whole is stirred 'energetically and left to stand at the ordinary temperature for about ten to twelve hours. At

the end of this time the liquid is filtered, the

residue pressed out,-and the extraction renewed I with from one hundred-and fifty to two hunured liters of water aci'dulated with a liter of hydrochloric acid. The two extracts are mixed, and while stirring'there are added to them several materials hereinafter mentioned in aqueous solution. To the extract there is first added in the following order anaqueous solution of three thousand grams of ordinary crystallized copper sulfate. To this is added five hundred grams of calcium chlorid, then three thousand grams of anhydrous sodium acetate, and finally one thousand grams of dium hydroxid, (sods-lye.) The quantity of calcium chlorid can be greatlydiminished if the cakes to be treated for example, colza cakeare naturally rich in calcium salts, and in the latter event two hundred grams of calcium chlorid will sufiice. After this treatment the liquid retains an acid reaction, and a rich precipitateof a blue-green color is formed. This precipitate consists of a mixture of the double salts of the organic compound of phosphorus,

to a syrupy consistency in avacuum and prccipitated withtwo volumes of alcohol of ninetyfive proof or the syrup is directly evaporated to dryness and the dry materialpulverized. In this way, according to the nature of the cakes employed, from two thousand five hundred.

to three thousand five hundred grams of a white powder is obtained, which is perfectly soluble in water, is free from inorganic phosphates, and contains more than twenty per cent. of its own weight of phosphorus.

It is obviousthat instead of soda-lye potash lye may be employed without appreciably altering the result, and instead of calcium chlorid another. soluble calcium salt, instead of hydrochloric'acid any other mineral acid, and, likewise, instead of copper sulfate any other salt of copper, lead, or analogous metal, and instead of sodium acetate any other suitable alkali acetate may be used.

The product obtained by the process above described shows the above-mentioned proporture and physiological action it is assimilable and may be employed as nourishment.

Over known processes the method abovedescribed has many advantages, owing to the fact that the process involves only employment of a cheap and easily accessible materialviz., oil'cakes-also that this process, owing to the employment of the mineral acids used asextracting media, renders it practicable to obtain seventy-five to eighty per cent. of the phosphorus contained in the initial material in the form of the organic compound above defined, an output which by far exceeds any, that has been previously obtainable.

Again, this process is directly applicable to' the production of extracts free from albumen, and thereby enables me to avoid the tedious and time -wasting operations of coagulating and filtering the protein substances. Lastly, the product obtained according to this process is free from every organic impurity. This last-mentioned advantage is, indeed, obvious, since the proportion of phosphorus contained in the product which is prepared by this method is considerably higher than the proportion of phosphorus containedin other kindred substances that have been treated hitherto.

Having thus described my invention, 1 claimi l. The herein-described process for obtaining the assimilable phosphorus compound contained in most vegetable foodstufi's and especially in oil-cake, consisting in suitably comminuting the vegetable material, treating the comrninuted vegetable material with an alkali lye in order to loosen-the aleurone bodies, treating further the mass with a dilute mineral acid, filtering and mixing the filtered liquid with a heavy metal salt, a salt of an alka line earth, an alkaline salt of an organic acid, and an alkaline substance, in order to precipitate the phosphorus compound in presenceof a free organic acid in the form of double salts of alkaline earths and heavy metals, treating a suspension of .the said double salts in water. with hydrogen sulfid and filtering-tor removing the heavy metal as sulfid, and finally evaporating the filtered liquid.

2. The herein-described process for obtaining the assimilable phosphorus compound contained in most vegetable foodstuffs and especially in oil-cake, consisting in treating the vegetable material with a dilute mineral acid, filtering and mixing the filtered liquid, witha. heavy metal salt, a salt of an alkaline earth, an alkaline salt of an organic acid and an a1- kaline substance, in order 10 precipitate the' phosphorus compound in presence of a free l organic acid in the form of double salts of all-taline earths a nd heavy metals, treating a sushydrogen sulfid and filtering for removing the heavy metal as sulfid, and tinally evaporating the filtered liquid.

3. The hereimdcseribed process for obtaining the assimilable phosphorus compound contained in inc -1 vegetable foodstuffs and especially in oil ike, consisting ininixing an extract of the egetable material in a'mineral acid with a ,heavy metal salt, a salt of an alkaline earth and an alkaline salt of an organic acid and an alkaline substance, in order to precipitate the phosphorus compound, in presence ofa free organic acid, in the form of double salts of alkaline earths and heavy metals, treating a suspension of the said double salts in water with hydrogen sulfid and filterand finally evaporating the filtered liquid.

4. The herein-described procem for obtainin g the assimilable phosphorus compound contained in most vegetable focxlstufisand cspe cially in oil-cake, consisting in treating a suscornpound with-alkaline earths and heavy metals with hydrogen sulhd, filtering for removevaporating the filtered liquid.

5. The herein-described process for obtaining the assimilable' phosphorus compound contained in most v getable foodstuffs, and especially in oil-cake, consisting in trcatinga suspension of double salts of the said phosphorus compound with alkaline earths and heavy metals with hydrogen sultid, filtering for removing the precipitated metal suliid, evaporating the filtered liquid to a syrupy consistency, precipitating the alcohol, drying, and finally pulverizing. a

6. As a new article of manufacture, the here-. in-described mixture of acid salts of the organic assirnilable phosphorus compound of vegetable 'foodstufis, cormspouding t0 the formula CiHdzOe, which constitutes, in dry state, a white powder, soluble in water, free from inorganic phosphates and containing more than twenty per cent. of its own weight of phosphorus.

In testimony whereof I have hereunto 'set my hand in the presence of two witnesses.

'SlYIbEL POSTERNAK. lvitncs esz 4 EDWARD P. MACLLAS;

J. ALLrsos Eon-rs.-

ing for removing the heavy metal as sullid,

pension of double salts of the said phosphorus pension of the said double salts in water with ing the precipitated metal sullid, and finally 

